KWAME NKRUMAH UNI VERSI TY OF SCI ENCE AND

TECHNOLOGY
DEPARTMENT OF CHEMI STRY
YEAR TWO (CHEM 269)
PRACTI CAL CHEMI STRY I I I
TITLE: STANDARDIZATION OF SOME VOLUMETRIC
GLASSWARE: A STATISTICAL STUDY
NAME: OPOKU ERNEST
EMAIL: [email protected]
DATE: 20
TH
OCTOBER, 2013
STANDARDI ZATI ON OF SOME VOLUMETRI C GLASSWARE:
A STATI STI CAL STUDY
AI MS AND OBJECTI VES:
1. To familiarize students with the use of the balance.
2. To develop the proper technique for the use of volumetric glassware.
3. To introduce the proper procedures for keeping a laboratory notebook.
4. To apply statistical analysis to real set of data.
5. To begin instruction on the use of the computer for data analysis, in this case using
spreadsheet program.
6. To teach the procedure for standardizing volumetric glassware.
I NTRODUCTI ON:
There are three main types of containers used in the lab to deliver or contain liquids:
volumetric, ordinary, and disposable glassware.
Volumetric glassware are containers that have calibrated at a specific temperature to deliver
or contain very precise amount of liquid. Examples of volumetric glassware are burette,
pipette, volumetric flask and the like.
Ordinary glassware has less precise volume calibration and is used whenever the volume
does not have to be measured as accurately. Examples include beakers, Erlenmeyer flask, and
graduated cylinder.
Disposable glassware (or plastic ware) is used to transfer or hold liquids temporarily and may
not contain any volume marking, examples include medicine droppers and disposable pipette.
In this experiment we will be exposed to a variety of important concepts related to
quantitative experimentation, including the proper use of glassware, analytical balance, and
statistics.
We will calibrate a volumetric pipette or flask that is we will experimentally determine what
volume a pipette or a flask really delivers. We will also calibrate a beaker.
Titrimetric analysis methods heavily utilize solution chemistry, and therefore volumes of
solutions are prepared, measured, transferred, and analysed with some degree of frequency in
this type of analysis. There is therefore the need to be versed in the selection and proper use
of the glassware and devices used for precise volume measurement.
Precision is the repeatability of a measurement whiles accuracy refers to the correctness of a
measurement or how close it comes to the correct value of a parameter; these are of optimum
interest in any analysis as no quantitative results are of any value unless they are
accompanied by some estimate of errors inherent in them.
Temperature (
0
C) Density (g/mL)
11 0.9996084
12 0.9995004
13 0.9993801
14 0.9992474
15 0.9991026
16 0.9989460
17 0.9987779
18 0.9985986
19 0.9984082
20 0.9982071
21 0.9979955
22 0.9977735
23 0.9975415
24 0.9972995
25 0.9970479
26 0.9967867
27 0.9965162
28 0.9962365
29 0.9959478
30 0.9956502
Calibration of the instrument to be used in an analysis increases the precision and the
accuracy of the results by determining the relationship between the analytical response and
the analyte concentration. Calibration refers to a procedure that checks the device to confirm
that it provides the known value.
Most pipettes are pieces of glassware that are designed to deliver the indicated volume.
Pipettes come in a variety of sizes and shapes. The most common is probably the volumetric
pipette, or transfer pipette. The transfer pipette is calibrated in units to deliver volumes
ranging from 0.1 to 25ml whiles the volumetric pipette deliver specific volumes of solution.
Measuring cylinders are used in measuring varying volumes of solution. The experiment is to
determine whether a 10ml pipette and a 10ml measuring cylinder deliver the said volumes of
solution.
.
CHEMI CALS AND EQUI PMENT
1. Distilled water
2. Electronic balance, model: Adventurer Pro AV812, S/N: 1126492837.
3. 100ml volumetric flasks
4. 10ml pipette
5. 10ml measuring cylinder
6. Beaker
PROCEDURE
1. An empty volumetric flask was weighed on an electronic balance and the weight
recorded as M1.
2. 100ml of water was then poured into it for reweighed and the new weight measured as
M2.
3. This experiment was repeated twice and their corresponding weight are recorded.
4. The experiment was repeated using the measuring cylinder and the beaker.
5. The actual weight of water contained in each case is noted down.
TABLE OF RESULTS
STANDARDI ZATI ON OF PI PETTE (10ML)
Mass of empty volumetric flask + stopper (W1) = 54.99 g
Room temperature of water in flask = 28.3
o
C
Density of water at 28.3
o
C= 0.995944g/ml
Volume of water
in (mL)
W2 in grams (W2-W1)in grams Actual weight of
water (per 10ml)
in grams
Actual volume of
water measured
in ml (V)
10 64.81 9.82 9.82 9.86
20 74.69 19.70 9.88 9.92
30 84.60 29.61 9.91 9.95
40 94.53 39.54 9.93 9.97
50 104.40 44.91 9.87 9.91
60 114.33 59.34 9.93 9.97
70 124.26 69.27 9.93 9.97
80 134.08 79.07 9.82 9.86
90 144.01 89.02 9.93 9.97
100 153.97 98.98 9.96 10.00
Mean mass of water = 2(9.82) + (9.88) + 4(9.93) + 9.87 + 9.96 + 9.91 = 9.898g
10
mean volume of water ( ) = 2(9.86) + 9.92 + 9.95 + 4(9.97) + 9.91 + 9.86 = 9.924mL
10
V- (mL) [V- ]
2
-0.064 0.004096
-0.004 0.000016
0.026 0.000676
0.046 0.002116
-0.014 0.000196
0.046 0.002116
0.046 0.002116
-0.064 0.004096
0.046 0.002116
0.076 0.005776
Standard deviation =
[ ]
= 0.00232/9 = 0.05
Average deviation, d = [ ]/ =0.496/10 = 0.0496
Relative error = (10- 9.924)/10 100 = 0.76%
Relative Standard Deviation = s 100 = 0.05/9.924 100 = 0.50%
Relative Average Deviation = d 100 = 0.0496/9.924 100 = 0.499%
The value of t at 90% and 95% confidence limits are 1.833 and 2.262 respectively.
At 90% confidence, confidence limit = 9.924 1.833(0.05)/10 = 9.924 0.030
= 9.894- 9.954
at 95% confidence, confidence limit = 9.924 2.262(0.05)/10 = 9.924 0.036
= 9.888- 9.960
STANDARDI ZATI ON MEASURI NG CYLI NDER (10ML)
Mass of empty volumetric flask + cork = 53.96g
temperature of water in flask = 27.6
o
C
density of water at 27.6
o
C= 0.996232g/ml
Volume of water
in ml
W2 in grams (W2-W1) in
grams
Actual weight of
water (per 10ml)
in grams
Actual volume of
water measured
in ml (V)
10 63.92 9.96 9.96 9.99
20 73.67 19.71 9.75 9.79
30 84.43 29.47 9.76 9.80
40 93.16 39.20 9.73 9.77
50 102.84 48.88 9.68 9.72
60 112.50 58.60 9.72 9.76
70 122.40 68.44 9.84 9.88
80 132.08 78.12 9.68 9.72
90 141.87 87.91 9.79 9.83
100 151.64 97.68 9.77 9.81
Mean mass of water = 9.96 + 9.75 + 9.76 + 9.73 + 9.68 +9.72+9.84+9.68+9.79+9.77 =
9.768g
10
Mean volume of water ( )=9.99 + 9.79 + 9.80 + 9.77 +2( 9.72) + 9.76 + 9.88+9.83+9.81=
9.807g
10
V- [V- ]
2
0.183 0.033489
-0.017 0.000289
-0.007 0.000049
-0.037 0.001369
-0.087 0.007569
-0.047 0.002209
0.073 0.005329
-0.087 0.007569
0.023 0.000529
0.003 0.000009
[ ] = 0.15 [ ]
2
= 4.0910
-3
Standard deviation = 0.00409/9 = 0.0213
Average deviation = 0.15/10 = 0.015
Relative error = (10- 9.889)/10100 = 1.11%
Relative Standard Deviation = 0.0213/9.889 100 = 0.215%
Relative Average Deviation = 0.015/9.889 100 = 0.152%
At 90% confidence, confidence limit = 9.889 1.833(0.0213)/10 = 9.889 0.0123
= 9.8767-9.9013
at 95%confidence, confidence limit = 9.889 2.262(0.0213)/10 = 9.889 0.0152
= 9.8738- 9.9042
DI SCUSSI ON
According to the results it can be noted that the actual volumes calculated were not equal to
the volumes predicted. The actual volumes were less than the predicted volumes. This could
be due to errors. The results of the instruments can be reported as;
99.130.151 for volumetric flask at 90% confidence limit29.76ml 0.0276 for the pipette at
90% confidence limit
9.72ml 0.245 for the measuring cylinder at 90% confidence limit
All the instruments were not precise in the experiment conducted, for precision is the
repeatability or reproducibility of measured values of the same quantity. This evidence is
found in all the results of the instruments example; none of the values were repeated twice in
the data collected during the experiment. However the data of the experiment were not
accurate because none had a range equal to or above the true value of the volumetric
glassware standardized.
PRECAUTI ON
1. All glassware were thoroughly clean before the start of the actual experiment.
Cleanliness of glassware is of important, if films or dirt grease are present liquids will
not drain uniformly and will leave water breaks or droplets on the walls. Under such
condition the calibration will be in error.
2. Reading from all the measuring glassware were taken at the eye level to avoid parallax
error.
3. The water left at the tip of the pipette was not blown out into the rest of the solution.
4. The volume of the solution was read below the meniscus.
5. The electronic balance was calibrated before use.
ERROR ANALYSI S
The errors encountered during the experiment were due to the change in temperature of the
surrounds and the system. For each of the glassware were mark with a specific temperature
that it can operate to give the accurate volume readings for the glassware studied in this
experiment. Dirt and grease on the inner glass surface prevents liquid from draining evenly
leaving droplets of the liquid less than the calibrated volumes. Though the pipette and all the
other equipment used in the experiment were rinsed with distilled water before they were
used, dirt and grease are insoluble in water and could have caused such an error. Also every
volume measuring instrument is supposed to have a run-down time which is the time taken
for the liquid been measured to drain totally from the device. However, this was not obeyed
as there was very limited time for the experiment to be carried out, hence leaving some of the
liquid in the measuring device.
CONCLUSI ON
The various volumes allocated to the pipette and measuring cylinders were compared to the
results obtained after the experiment.
Students can now independently use the electronic balance for all manipulations it is
expected. Proper technique was achieved on how to read volume on volumetric glassware.
Even though it was observed that volume of the various standardized glassware was not
accurate , this to tell us that glassware in the various laboratory may not accurately contain
the volume prescribe on them unless the parameter s like temperature and density of the
substance are noted .
REFERENCES
1. Statistics for Analytical Chemistry, J.C. Miller and J.N. Miller, 3
rd
edition, page 16-20
2. Vogels hand text book of Quantitative chemical analysis ,fifth edition, G.H. Jeffery,
J.Bassett, J.Mendham.pg 40-45
3. Analytical chemistry for Technicians, John Kenkel, 3
rd
edition, page 12
4. Skoog- Fundamentals of Analytical Chemistry, 8
th
edition, page 40, 41, 129